反应详情

温度

0 °C

To a solution of Compound 241 (1.2 g, 1.81 mmol) obtained in Example 242 in 25 ml of N,N-dimethylformamide was portionwise added sodium hydride (60% in oil, 160 mg, 3.81 mmol) with stirring at 0° C., and 2-dimethylaminoethylchloride hydrochloride (260 mg, 1.81 mmol) was added thereto, followed by heating to 80° C. and then stirring for 7 hours. A saturated aqueous solution of ammonium chloride was added to the reaction solution for neutralization, and water was added thereto followed by extraction with ethyl acetate. The resulting organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure to give a crude product. The obtained crude product was purified with silica gel column chromatography (ethyl acetate/hexane=2/1) to give 1.1 g (yield: 85%) of the title compound.

1. temperatureby heating to 80° C.
2. stirringstirring for 7 hours
3. additionwas added
4. extractionthereto followed by extraction with ethyl acetate
5. washThe resulting organic layer was washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over magnesium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. customto give a crude product
9. customThe obtained crude product
10. customwas purified with silica gel column chromatography (ethyl acetate/hexane=2/1)